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Lost During First Extraction - help wanted

I

its0x11

Rising Star
Merits
177
Alright so here's the deal. I'm doing my first extraction from Svrian Rue seeds. I'm following the Tek on the Nexus located here:

Harmalas Extraction and Separation Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me wiki.dmt-nexus.me

Please don't beat me up, but it was the only
one I found when I was starting.

Here's what I've done so far, please bear with me, but I'm stuck and didn't end up with needle crystals like I expected when I'm done with step 13.
I took 200g of seeds, acid boiled 4 times with vinegar water. Discarded the seeds when it was done and collected about 4L of tea. I did a low simmer for several hours and reduced the 4L to approximately 1L of concentrated tea. After it cooled, I added some lye until it turned milky.
I tested the PH the next day and it was around 12. After the media bottle cooled down, I put it in the fridge overnight and through the next work day, about 20 hours
probably.

This separated into clear red liquid on top and brown condensate liquid on the bottom. I poured off the red and ran the brown through coffee filters and collected the brown back into my pan, redissolved the brown into vinegar and water, it ends up being right at 2.5L of liquid at this point because I had to
add so much vinegar to dissolve the majority of the material. It was a PH of iust under 5 at this point.

I ran the acidic solution through coffee filters 3 times to filter out undissolved plant material.

At this point, I put it back into the pan, got it to a low boil and added 240g of salt. stirred until the salt dissolved and poured it back into the bottles.

After the bottles cooled to room temp, I put them in the refrigerator overnight

At this point, I should have crystals on the bottom right?
I have sludge again. I'm running it through the coffee filters to try collecting it to dissolve in water for the next step, but it feels like l've done something wrong at this point
Adding pics here, pic 1 is the red basic liquid left after the first crash and separation. Pic 2 is me straining the acidic salt solution after precipitating overnight. Pic 3 is the
sludge I'm left with in my filters I will also note that everything is fluorescing either yellow, green or blue under UV, even the remaining basic solution, so I have alkaloids everywhere
Thanks for helping out. I've watched several videos and they're iust making the process more confusing at this point and I can't find an appropriate answer.
 

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its0x11 said:
I poured off the red and ran the brown through coffee filters and collected the brown back into my pan, redissolved the brown into vinegar and water, it ends up being right at 2.5L of liquid at this point because I had to
add so much vinegar to dissolve the majority of the material. It was a PH of iust under 5 at this point.
Click to expand...
Imo you have added too much vinegar water during redissolving your brown precipitate, now it is too diluted to properly crystalize.
My advice is too basify it again by adding some lye and let harmalas precipitate. Continue then as planned but do not dilute it again so much.
 
doubledog said:
Imo you have added too much vinegar water during redissolving your brown precipitate, now it is too diluted to properly crystalize.
My advice is too basify it again by adding some lye and let harmalas precipitate. Continue then as planned but do not dilute it again so much.
Click to expand...
So when I redissolve it with vinegar, should I worry about the PH at all? When I did it the first time, it took a lot of vinegar and water to get it down below a 6 even.
 
doubledog said:
Imo you have added too much vinegar water during redissolving your brown precipitate, now it is too diluted to properly crystalize.
My advice is too basify it again by adding some lye and let harmalas precipitate. Continue then as planned but do not dilute it again so much.
Click to expand...
Also, should I put the sludge and acid salt solution back together and basify with lye on all of it or leave anything filtered out from where I am now?
 
its0x11 said:
I poured off the red and ran the brown through coffee filters and collected the brown back into my pan, redissolved the brown into vinegar and water, it ends up being right at 2.5L of liquid at this point because I had to
add so much vinegar to dissolve the majority of the material. It was a PH of iust under 5 at this point.
Click to expand...
Yeah as doubledog mentioned the problem is in adding too much acid and water and getting it too dilute. The thing is that not everything is expected to dissolve, especially after only the first A/B cycle, there are impurities and they do seem a lot like just moar harmala alkaloids but they're not. So they should be filtered out and one should not try to keep adding acid, once the solution becomes acidic that is enough (as long as it is not super concentrated) the harmalas are very soluble in acidic water they will quickly dissolve. In later A/B cycles you can expect everything to dissolve but often some stuff or cloudiness remains, and it's a good opportunity to try and filter it out.

The simplest course or action is again as doubledog said, to base it and collect the precipitate. Redissolve in acidic water, perhaps aiming for 300 ml total volume would be appropriate. And this time after making sure the solution is acidic, filter out any undisolved materil. Then proceed with the manske step keeping the volumes low.
 
Sakkadelic said:
Yeah as doubledog mentioned the problem is in adding too much acid and water and getting it too dilute. The thing is that not everything is expected to dissolve, especially after only the first A/B cycle, there are impurities and they do seem a lot like just moar harmala alkaloids but they're not. So they should be filtered out and one should not try to keep adding acid, once the solution becomes acidic that is enough (as long as it is not super concentrated) the harmalas are very soluble in acidic water they will quickly dissolve. In later A/B cycles you can expect everything to dissolve but often some stuff or cloudiness remains, and it's a good opportunity to try and filter it out.

The simplest course or action is again as doubledog said, to base it and collect the precipitate. Redissolve in acidic water, perhaps aiming for 300 ml total volume would be appropriate. And this time after making sure the solution is acidic, filter out any undisolved materil. Then proceed with the manske step keeping the volumes low.
Click to expand...
Rebase the liquid and sludge together or just the liquid and leave the sludge filtered at the point I am right now?
 
Sakkadelic said:
Yeah i'd say rebase everything it's not clear where the harmalas are in your case, whether they crashed out or stayed dissolved or both. Is the sludge at all shiny?
Click to expand...
Here's 3 funnels containing everything I filtered out, it's fluorescing for sure.
 

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Sakkadelic said:
If you have them already seperate that's nice, you can process each seperately and combine the liquids after acidification and filtering.
Click to expand...
That's a great idea. I'll do that. I'll report back tomorrow after I try all of this again. I appreciate it. I really need to buy a vacuum filtration system and diaphragm pump to speed some of these steps up.
 
That would be nice but it's really not needed, the easy direction with harmala extraction is keeping the seeds whole and leaving the fine filtering till the end. Rely on settling, decanting, and washing to clean the harmalas and filtration at the end to finish the job.
 
Sakkadelic said:
That would be nice but it's really not needed, the easy direction with harmala extraction is keeping the seeds whole and leaving the fine filtering till the end. Rely on settling, decanting, and washing to clean the harmalas and filtration at the end to finish the job.
Click to expand...
Guess I need to follow a different Tek then. The one I linked has you filtering for days.
 
Here's some recent versions of the simpler harmala extraction path

q21q21

TEK Thread 'Speedy No-Filter Harmalas Tek (draft)'

Speedy No-Filter Harmalas Tek

*Splash Picture of all steps*

The core ideas in this tek are based on the posts by Ouro/Mydriasis, Brennendes Wasser & Gibran2

As with “my” DMT tek, I’m simply standing on the shoulders of giants and breaking down a method as comprehensively as I can for clarity.

The inspiration for writing this “tek” is the no-filter strategy that replacing filtration with several washing and decanting steps.

With the exception of Gibran2’s tek on the wiki which explicitly advises against using Syrian Rue, the threads which mention this method...
  • Like
  • Love

Orion

Thread 'Rue to separated freebases with less fuss.'

Here I've combined elements from very conveniently simplified approaches by Sakkadelic and Brennendes Wasser into one method. I've reworked a couple of details, removed some unnecessary steps and added quick and easy salt and optional separation stages. In my opinion this is an easy, quick way to separated Harmine and Harmaline freebase of reasonable purity and good yields without grinding of seeds or filtering and reducing of large volumes of water. No funnels, no cotton balls and no extra back and forth between acids and bases.

Materials:

100G of dry Syrian...
  • Like
  • Love
  • Care

And i've also recently tried cwe although with ground seeds but it is still mess free.

Sakkadelic

Thread 'Harmala CWE experiment'

Recently, inspired by blig-blug's success with mimosa CWE I wanted to try the same with rue for the purpose of daily harmala use. But then I thought if it is effective, it makes sense to use it for harmala extraction, no more hours of smelly rue cooking and no messy filtration, it would take a few days to complete but the effort is much reduced. CWE doesn't make as much sense for dmt extractions because of the large water volume and we already have STB.
I will first outline the general steps and then go in more details about what I did in this first experiment and the results I got...
  • Like
  • Love
 
Sakkadelic said:
Here's some recent versions of the simpler harmala extraction path

q21q21

TEK Thread 'Speedy No-Filter Harmalas Tek (draft)'

Speedy No-Filter Harmalas Tek

*Splash Picture of all steps*

The core ideas in this tek are based on the posts by Ouro/Mydriasis, Brennendes Wasser & Gibran2

As with “my” DMT tek, I’m simply standing on the shoulders of giants and breaking down a method as comprehensively as I can for clarity.

The inspiration for writing this “tek” is the no-filter strategy that replacing filtration with several washing and decanting steps.

With the exception of Gibran2’s tek on the wiki which explicitly advises against using Syrian Rue, the threads which mention this method...
  • Like
  • Love

Orion

Thread 'Rue to separated freebases with less fuss.'

Here I've combined elements from very conveniently simplified approaches by Sakkadelic and Brennendes Wasser into one method. I've reworked a couple of details, removed some unnecessary steps and added quick and easy salt and optional separation stages. In my opinion this is an easy, quick way to separated Harmine and Harmaline freebase of reasonable purity and good yields without grinding of seeds or filtering and reducing of large volumes of water. No funnels, no cotton balls and no extra back and forth between acids and bases.

Materials:

100G of dry Syrian...
  • Like
  • Love
  • Care

And i've also recently tried cwe although with ground seeds but it is still mess free.

Sakkadelic

Thread 'Harmala CWE experiment'

Recently, inspired by blig-blug's success with mimosa CWE I wanted to try the same with rue for the purpose of daily harmala use. But then I thought if it is effective, it makes sense to use it for harmala extraction, no more hours of smelly rue cooking and no messy filtration, it would take a few days to complete but the effort is much reduced. CWE doesn't make as much sense for dmt extractions because of the large water volume and we already have STB.
I will first outline the general steps and then go in more details about what I did in this first experiment and the results I got...
  • Like
  • Love
Click to expand...
Thanks for these. So let me just kinda clarify my next steps. Right now, I've rebasified. I have 3 media bottles with ~700ml each of milky brown liquid. I have 1 flask with ~300ml of milky brown sludge. After reading the linked posts, I can likely decant these bottles and flask tomorrow morning and then do 4 or 5 simple water washes since it should all be free base at this point. Once I've decanted the washes several times and I'm left with more sludge, I should just dry it if I want freebase? Or should I run it through another A/B cycle at that point to clean it up more?

My end goal is to end with the salts so I can make a nasal spray for easy daily use at some lower dosages.
 

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